Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807026013/zl2034sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807026013/zl2034Isup2.hkl |
CCDC reference: 654706
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.002 Å
- R factor = 0.038
- wR factor = 0.110
- Data-to-parameter ratio = 12.0
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 200 Deg. PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.47 PLAT417_ALERT_2_C Short Inter D-H..H-D H1A .. H5W .. 2.13 Ang. PLAT417_ALERT_2_C Short Inter D-H..H-D H2W .. H6W .. 2.14 Ang.
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 9
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
The title complex was prepared by the addition of 5-aminoisophthalic acid to a hot aqueous solution. The pH was then adjusted to 7.0 to 8.0 with NaOH (0.1 mol/L). The resulting solution was filtered, and colourless crystals were obtained at room temperature on slow evaporation of the solvent over several days.
Carbon-bound H atoms were placed at calculated positions and were treated as riding on the parent C atoms with C—H = 0.93 Å, N—H = 0.96 Å and with Uiso(H) = 1.2 Ueq(C) and 1.5 Ueq(N). Water H atoms were tentatively located in difference Fourier maps and were refined with distance restraints of O–H = 0.82 Å and H···H = 1.29 Å, each within a standard deviation of 0.01 Å, and Uiso(H) = 1.5 Ueq(O).
Molecular self-assembly of supramolecular architectures has received much attention during recent decades (Kim et al., 2003; Iglesias et al., 2003; Moulton & Zaworotko, 2001). The structures and properties of such systems depend on the coordination and geometric preferences of both the central metals ions and bridging building blocks as well as the influence of weaker non-covalent interactions, such as hydrogen bonds and π-π stacking interactions.
As illustrated in Fig. 1, in the dinuclear centrosymmetric structure of (I) each NaI centre is coordinated by three carboxyl O atoms from three 5-aminoisophthalato ligands, and three water molecules. In the distorted octahedral geometry each of the water molecules is located trans to a carboxyl O atom (Table 1). The Na···Na separation within the centrosymmetric dinuclear complex is 10.251 (3) Å, and the the two central 5-aminoisophthalato ligands are parallel to each other at a plane to plane distance of about 3.43 Å, thus indicating a π stacking interaction (Fig 1). The structure is further extended to a supramolecular network through intra and intermolecular N—H···O and O—H···O hydrogen bonding interactions (Fig 2., Table 2).
For related literature, see: Iglesias et al. (2003); Kim et al. (2003); Moulton & Zaworotko (2001).
Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2004); software used to prepare material for publication: SHELXTL.
[Na2(C8H6NO4)2(C8H7NO4)2(H2O)6] | Z = 1 |
Mr = 876.64 | F(000) = 456 |
Triclinic, P1 | Dx = 1.618 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.1889 (3) Å | Cell parameters from 3500 reflections |
b = 8.8821 (3) Å | θ = 1.7–26.0° |
c = 12.6381 (5) Å | µ = 0.16 mm−1 |
α = 95.251 (2)° | T = 293 K |
β = 98.649 (2)° | Block, colourless |
γ = 95.200 (2)° | 0.19 × 0.16 × 0.15 mm |
V = 899.86 (6) Å3 |
Bruker APEXII area-detector diffractometer | 2714 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.029 |
Graphite monochromator | θmax = 26.0°, θmin = 1.6° |
φ and ω scans | h = −10→10 |
11809 measured reflections | k = −10→10 |
3506 independent reflections | l = −15→14 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.038 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.110 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0543P)2 + 0.2242P] where P = (Fo2 + 2Fc2)/3 |
3506 reflections | (Δ/σ)max = 0.001 |
292 parameters | Δρmax = 0.24 e Å−3 |
9 restraints | Δρmin = −0.22 e Å−3 |
[Na2(C8H6NO4)2(C8H7NO4)2(H2O)6] | γ = 95.200 (2)° |
Mr = 876.64 | V = 899.86 (6) Å3 |
Triclinic, P1 | Z = 1 |
a = 8.1889 (3) Å | Mo Kα radiation |
b = 8.8821 (3) Å | µ = 0.16 mm−1 |
c = 12.6381 (5) Å | T = 293 K |
α = 95.251 (2)° | 0.19 × 0.16 × 0.15 mm |
β = 98.649 (2)° |
Bruker APEXII area-detector diffractometer | 2714 reflections with I > 2σ(I) |
11809 measured reflections | Rint = 0.029 |
3506 independent reflections |
R[F2 > 2σ(F2)] = 0.038 | 9 restraints |
wR(F2) = 0.110 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.06 | Δρmax = 0.24 e Å−3 |
3506 reflections | Δρmin = −0.22 e Å−3 |
292 parameters |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
C1 | 0.1175 (2) | 0.2786 (2) | 1.00350 (14) | 0.0251 (4) | |
C2 | 0.0923 (2) | 0.16994 (19) | 1.08453 (14) | 0.0233 (4) | |
C3 | 0.2264 (2) | 0.0955 (2) | 1.12436 (14) | 0.0253 (4) | |
H3 | 0.3292 | 0.1168 | 1.1031 | 0.030* | |
C4 | 0.2060 (2) | −0.01048 (19) | 1.19577 (14) | 0.0241 (4) | |
C5 | 0.0531 (2) | −0.04674 (19) | 1.22571 (14) | 0.0242 (4) | |
H5 | 0.0403 | −0.1214 | 1.2717 | 0.029* | |
C6 | −0.0814 (2) | 0.02815 (19) | 1.18715 (14) | 0.0230 (4) | |
C7 | −0.0614 (2) | 0.13772 (19) | 1.11621 (14) | 0.0237 (4) | |
H7 | −0.1507 | 0.1890 | 1.0902 | 0.028* | |
C8 | −0.2484 (2) | −0.0130 (2) | 1.22114 (14) | 0.0247 (4) | |
C9 | −0.0748 (2) | 0.5059 (2) | 0.74424 (15) | 0.0288 (4) | |
C10 | −0.0515 (2) | 0.60556 (19) | 0.65623 (14) | 0.0237 (4) | |
C11 | −0.1875 (2) | 0.6705 (2) | 0.60714 (14) | 0.0252 (4) | |
H11 | −0.2909 | 0.6513 | 0.6279 | 0.030* | |
C12 | −0.1679 (2) | 0.76336 (19) | 0.52771 (14) | 0.0228 (4) | |
C13 | −0.0155 (2) | 0.79463 (19) | 0.49608 (14) | 0.0242 (4) | |
H13 | −0.0042 | 0.8585 | 0.4427 | 0.029* | |
C14 | 0.12133 (19) | 0.72997 (19) | 0.54466 (14) | 0.0234 (4) | |
C15 | 0.1019 (2) | 0.63570 (19) | 0.62487 (14) | 0.0246 (4) | |
H15 | 0.1930 | 0.5924 | 0.6578 | 0.030* | |
C16 | 0.2881 (2) | 0.7633 (2) | 0.50918 (15) | 0.0258 (4) | |
N1 | 0.34825 (17) | −0.08917 (17) | 1.23537 (13) | 0.0293 (4) | |
H1A | 0.3487 | −0.1741 | 1.1922 | 0.044* | |
H1B | 0.3411 | −0.1124 | 1.3017 | 0.044* | |
H1C | 0.4417 | −0.0291 | 1.2364 | 0.044* | |
N2 | −0.31119 (17) | 0.83326 (16) | 0.47749 (12) | 0.0264 (3) | |
H2A | −0.4044 | 0.7823 | 0.4892 | 0.040* | |
H2B | −0.3106 | 0.8305 | 0.4070 | 0.040* | |
H2C | −0.3056 | 0.9294 | 0.5058 | 0.040* | |
Na1 | 0.32524 (8) | 0.39379 (8) | 0.81767 (6) | 0.0301 (2) | |
O1 | 0.25624 (15) | 0.31616 (16) | 0.98325 (11) | 0.0368 (4) | |
O2 | −0.01689 (14) | 0.32523 (15) | 0.95567 (11) | 0.0339 (3) | |
H2 | 0.0044 | 0.3713 | 0.9052 | 0.051* | |
O3 | −0.26498 (14) | −0.13253 (14) | 1.26574 (11) | 0.0322 (3) | |
O4 | −0.36025 (15) | 0.07342 (15) | 1.20278 (12) | 0.0395 (4) | |
O5 | 0.05126 (15) | 0.45954 (16) | 0.79542 (11) | 0.0371 (4) | |
O6 | −0.21793 (16) | 0.4762 (2) | 0.76354 (14) | 0.0593 (5) | |
O7 | 0.40436 (15) | 0.69099 (17) | 0.54356 (12) | 0.0427 (4) | |
O8 | 0.30116 (15) | 0.86535 (14) | 0.44630 (11) | 0.0314 (3) | |
O1W | 0.41376 (17) | 0.65365 (16) | 0.88767 (13) | 0.0410 (4) | |
O2W | 0.44720 (16) | 0.44095 (16) | 0.66516 (12) | 0.0386 (4) | |
O3W | 0.60029 (16) | 0.34300 (16) | 0.89387 (12) | 0.0373 (4) | |
H1W | 0.394 (2) | 0.7293 (17) | 0.8580 (17) | 0.045* | |
H4W | 0.5484 (12) | 0.447 (2) | 0.6801 (17) | 0.045* | |
H6W | 0.618 (2) | 0.342 (2) | 0.9601 (8) | 0.045* | |
H3W | 0.430 (2) | 0.5095 (19) | 0.6268 (16) | 0.045* | |
H2W | 0.5147 (12) | 0.662 (2) | 0.9063 (17) | 0.045* | |
H5W | 0.678 (2) | 0.402 (2) | 0.8828 (15) | 0.045* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0227 (9) | 0.0293 (9) | 0.0253 (10) | 0.0025 (7) | 0.0064 (7) | 0.0093 (8) |
C2 | 0.0221 (8) | 0.0267 (9) | 0.0227 (9) | 0.0019 (7) | 0.0060 (7) | 0.0081 (7) |
C3 | 0.0188 (8) | 0.0320 (10) | 0.0272 (10) | 0.0012 (7) | 0.0080 (7) | 0.0094 (8) |
C4 | 0.0196 (8) | 0.0292 (9) | 0.0256 (10) | 0.0062 (7) | 0.0046 (7) | 0.0088 (7) |
C5 | 0.0244 (9) | 0.0277 (9) | 0.0232 (10) | 0.0035 (7) | 0.0064 (7) | 0.0110 (7) |
C6 | 0.0202 (8) | 0.0265 (9) | 0.0234 (10) | 0.0012 (7) | 0.0062 (7) | 0.0064 (7) |
C7 | 0.0198 (8) | 0.0289 (9) | 0.0250 (10) | 0.0045 (7) | 0.0057 (7) | 0.0100 (7) |
C8 | 0.0197 (8) | 0.0336 (10) | 0.0225 (10) | 0.0017 (7) | 0.0059 (7) | 0.0096 (8) |
C9 | 0.0228 (9) | 0.0380 (11) | 0.0288 (10) | 0.0034 (7) | 0.0068 (7) | 0.0164 (8) |
C10 | 0.0209 (8) | 0.0285 (9) | 0.0235 (10) | 0.0023 (7) | 0.0045 (7) | 0.0114 (7) |
C11 | 0.0165 (8) | 0.0320 (9) | 0.0298 (10) | 0.0020 (7) | 0.0081 (7) | 0.0114 (8) |
C12 | 0.0179 (8) | 0.0266 (9) | 0.0252 (10) | 0.0052 (6) | 0.0034 (7) | 0.0080 (7) |
C13 | 0.0226 (8) | 0.0281 (9) | 0.0251 (10) | 0.0041 (7) | 0.0071 (7) | 0.0126 (7) |
C14 | 0.0191 (8) | 0.0293 (9) | 0.0243 (10) | 0.0037 (7) | 0.0073 (7) | 0.0093 (7) |
C15 | 0.0188 (8) | 0.0305 (9) | 0.0270 (10) | 0.0061 (7) | 0.0040 (7) | 0.0121 (8) |
C16 | 0.0192 (8) | 0.0327 (10) | 0.0287 (10) | 0.0041 (7) | 0.0087 (7) | 0.0104 (8) |
N1 | 0.0208 (7) | 0.0370 (9) | 0.0346 (9) | 0.0085 (6) | 0.0090 (6) | 0.0155 (7) |
N2 | 0.0203 (7) | 0.0315 (8) | 0.0309 (9) | 0.0071 (6) | 0.0074 (6) | 0.0131 (7) |
Na1 | 0.0243 (4) | 0.0364 (4) | 0.0333 (4) | 0.0055 (3) | 0.0091 (3) | 0.0139 (3) |
O1 | 0.0230 (7) | 0.0520 (9) | 0.0403 (9) | 0.0012 (6) | 0.0096 (6) | 0.0268 (7) |
O2 | 0.0253 (7) | 0.0444 (8) | 0.0382 (9) | 0.0081 (6) | 0.0090 (6) | 0.0269 (6) |
O3 | 0.0261 (7) | 0.0376 (8) | 0.0378 (8) | 0.0032 (5) | 0.0111 (6) | 0.0204 (6) |
O4 | 0.0219 (7) | 0.0433 (8) | 0.0612 (10) | 0.0099 (6) | 0.0156 (6) | 0.0261 (7) |
O5 | 0.0241 (7) | 0.0519 (9) | 0.0415 (9) | 0.0095 (6) | 0.0062 (6) | 0.0312 (7) |
O6 | 0.0203 (7) | 0.1007 (14) | 0.0673 (11) | 0.0035 (7) | 0.0110 (7) | 0.0613 (10) |
O7 | 0.0201 (7) | 0.0584 (9) | 0.0607 (10) | 0.0144 (6) | 0.0170 (6) | 0.0377 (8) |
O8 | 0.0275 (7) | 0.0370 (7) | 0.0362 (8) | 0.0061 (5) | 0.0150 (6) | 0.0191 (6) |
O1W | 0.0332 (7) | 0.0402 (8) | 0.0507 (10) | 0.0047 (6) | 0.0033 (7) | 0.0152 (7) |
O2W | 0.0291 (7) | 0.0446 (9) | 0.0455 (9) | 0.0031 (6) | 0.0092 (6) | 0.0189 (7) |
O3W | 0.0290 (7) | 0.0459 (9) | 0.0384 (9) | 0.0006 (6) | 0.0062 (6) | 0.0148 (7) |
C1—O1 | 1.225 (2) | C13—H13 | 0.9300 |
C1—O2 | 1.295 (2) | C14—C15 | 1.391 (2) |
C1—C2 | 1.494 (2) | C14—C16 | 1.513 (2) |
C2—C3 | 1.387 (2) | C15—H15 | 0.9300 |
C2—C7 | 1.391 (2) | C16—O7 | 1.243 (2) |
C3—C4 | 1.378 (2) | C16—O8 | 1.267 (2) |
C3—H3 | 0.9300 | N1—H1A | 0.8900 |
C4—C5 | 1.381 (2) | N1—H1B | 0.8900 |
C4—N1 | 1.460 (2) | N1—H1C | 0.8900 |
C5—C6 | 1.387 (2) | N2—H2A | 0.8900 |
C5—H5 | 0.9300 | N2—H2B | 0.8900 |
C6—C7 | 1.397 (2) | N2—H2C | 0.8900 |
C6—C8 | 1.518 (2) | Na1—O5 | 2.3520 (14) |
C7—H7 | 0.9300 | Na1—O2W | 2.3535 (16) |
C8—O3 | 1.253 (2) | Na1—O1 | 2.3922 (14) |
C8—O4 | 1.256 (2) | Na1—O1W | 2.4011 (16) |
C9—O6 | 1.242 (2) | Na1—O3W | 2.4115 (15) |
C9—O5 | 1.257 (2) | Na1—O3i | 2.4347 (15) |
C9—C10 | 1.507 (2) | O2—H2 | 0.8200 |
C10—C15 | 1.384 (2) | O3—Na1i | 2.4347 (15) |
C10—C11 | 1.390 (2) | O1W—H1W | 0.816 (9) |
C11—C12 | 1.374 (2) | O1W—H2W | 0.819 (9) |
C11—H11 | 0.9300 | O2W—H4W | 0.818 (9) |
C12—C13 | 1.379 (2) | O2W—H3W | 0.822 (9) |
C12—N2 | 1.465 (2) | O3W—H6W | 0.829 (9) |
C13—C14 | 1.391 (2) | O3W—H5W | 0.824 (9) |
O1—C1—O2 | 123.59 (16) | C14—C15—H15 | 119.6 |
O1—C1—C2 | 121.24 (15) | O7—C16—O8 | 123.72 (15) |
O2—C1—C2 | 115.14 (14) | O7—C16—C14 | 118.79 (15) |
C3—C2—C7 | 120.26 (15) | O8—C16—C14 | 117.48 (15) |
C3—C2—C1 | 117.75 (15) | C4—N1—H1A | 109.5 |
C7—C2—C1 | 121.93 (15) | C4—N1—H1B | 109.5 |
C4—C3—C2 | 119.41 (15) | H1A—N1—H1B | 109.5 |
C4—C3—H3 | 120.3 | C4—N1—H1C | 109.5 |
C2—C3—H3 | 120.3 | H1A—N1—H1C | 109.5 |
C3—C4—C5 | 121.02 (15) | H1B—N1—H1C | 109.5 |
C3—C4—N1 | 118.45 (14) | C12—N2—H2A | 109.5 |
C5—C4—N1 | 120.47 (15) | C12—N2—H2B | 109.5 |
C4—C5—C6 | 119.98 (15) | H2A—N2—H2B | 109.5 |
C4—C5—H5 | 120.0 | C12—N2—H2C | 109.5 |
C6—C5—H5 | 120.0 | H2A—N2—H2C | 109.5 |
C5—C6—C7 | 119.47 (15) | H2B—N2—H2C | 109.5 |
C5—C6—C8 | 119.25 (15) | O5—Na1—O2W | 110.25 (5) |
C7—C6—C8 | 121.27 (15) | O5—Na1—O1 | 82.66 (5) |
C2—C7—C6 | 119.81 (16) | O2W—Na1—O1 | 166.86 (6) |
C2—C7—H7 | 120.1 | O5—Na1—O1W | 87.51 (5) |
C6—C7—H7 | 120.1 | O2W—Na1—O1W | 87.97 (6) |
O3—C8—O4 | 124.40 (16) | O1—Na1—O1W | 95.25 (6) |
O3—C8—C6 | 117.05 (15) | O5—Na1—O3W | 163.62 (6) |
O4—C8—C6 | 118.55 (15) | O2W—Na1—O3W | 84.43 (5) |
O6—C9—O5 | 123.50 (16) | O1—Na1—O3W | 83.12 (5) |
O6—C9—C10 | 118.04 (15) | O1W—Na1—O3W | 85.74 (5) |
O5—C9—C10 | 118.45 (15) | O5—Na1—O3i | 97.80 (5) |
C15—C10—C11 | 119.60 (15) | O2W—Na1—O3i | 85.57 (5) |
C15—C10—C9 | 121.63 (15) | O1—Na1—O3i | 90.33 (5) |
C11—C10—C9 | 118.76 (15) | O1W—Na1—O3i | 172.76 (6) |
C12—C11—C10 | 119.53 (15) | O3W—Na1—O3i | 90.36 (5) |
C12—C11—H11 | 120.2 | C1—O1—Na1 | 127.35 (12) |
C10—C11—H11 | 120.2 | C1—O2—H2 | 109.5 |
C11—C12—C13 | 121.37 (15) | C8—O3—Na1i | 128.48 (12) |
C11—C12—N2 | 119.21 (14) | C9—O5—Na1 | 154.20 (12) |
C13—C12—N2 | 119.40 (15) | Na1—O1W—H1W | 127.1 (16) |
C12—C13—C14 | 119.52 (15) | Na1—O1W—H2W | 108.1 (14) |
C12—C13—H13 | 120.2 | H1W—O1W—H2W | 105.5 (13) |
C14—C13—H13 | 120.2 | Na1—O2W—H4W | 110.2 (15) |
C15—C14—C13 | 119.26 (15) | Na1—O2W—H3W | 126.7 (15) |
C15—C14—C16 | 121.28 (15) | H4W—O2W—H3W | 104.3 (13) |
C13—C14—C16 | 119.45 (15) | Na1—O3W—H6W | 115.8 (15) |
C10—C15—C14 | 120.72 (15) | Na1—O3W—H5W | 116.8 (15) |
C10—C15—H15 | 119.6 | H6W—O3W—H5W | 102.8 (13) |
Symmetry code: (i) −x, −y, −z+2. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···O3Wii | 0.89 | 1.89 | 2.763 (2) | 168 |
N1—H1B···O8iii | 0.89 | 1.93 | 2.810 (2) | 170 |
N1—H1C···O4iv | 0.89 | 1.91 | 2.7808 (19) | 165 |
N2—H2A···O7v | 0.89 | 1.94 | 2.8221 (18) | 169 |
N2—H2A···O8v | 0.89 | 2.58 | 3.1815 (18) | 126 |
N2—H2B···O3vi | 0.89 | 1.93 | 2.7981 (19) | 165 |
N2—H2C···O8vii | 0.89 | 1.86 | 2.750 (2) | 175 |
O2—H2···O5 | 0.82 | 1.73 | 2.5491 (17) | 177 |
O1W—H1W···O4viii | 0.82 (1) | 2.00 (1) | 2.8150 (19) | 175 (2) |
O2W—H4W···O6iv | 0.82 (1) | 2.02 (1) | 2.8128 (19) | 162 (2) |
O3W—H6W···O1Wix | 0.83 (1) | 1.98 (1) | 2.778 (2) | 162 (2) |
O2W—H3W···O7 | 0.82 (1) | 2.01 (1) | 2.8322 (19) | 174 (2) |
Symmetry codes: (ii) −x+1, −y, −z+2; (iii) x, y−1, z+1; (iv) x+1, y, z; (v) x−1, y, z; (vi) x, y+1, z−1; (vii) −x, −y+2, −z+1; (viii) −x, −y+1, −z+2; (ix) −x+1, −y+1, −z+2. |
Experimental details
Crystal data | |
Chemical formula | [Na2(C8H6NO4)2(C8H7NO4)2(H2O)6] |
Mr | 876.64 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 8.1889 (3), 8.8821 (3), 12.6381 (5) |
α, β, γ (°) | 95.251 (2), 98.649 (2), 95.200 (2) |
V (Å3) | 899.86 (6) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 0.16 |
Crystal size (mm) | 0.19 × 0.16 × 0.15 |
Data collection | |
Diffractometer | Bruker APEXII area-detector |
Absorption correction | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 11809, 3506, 2714 |
Rint | 0.029 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.038, 0.110, 1.06 |
No. of reflections | 3506 |
No. of parameters | 292 |
No. of restraints | 9 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.24, −0.22 |
Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2004), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 2004), SHELXTL.
Na1—O5 | 2.3520 (14) | Na1—O1W | 2.4011 (16) |
Na1—O2W | 2.3535 (16) | Na1—O3W | 2.4115 (15) |
Na1—O1 | 2.3922 (14) | Na1—O3i | 2.4347 (15) |
O5—Na1—O2W | 110.25 (5) | O1—Na1—O3W | 83.12 (5) |
O5—Na1—O1 | 82.66 (5) | O1W—Na1—O3W | 85.74 (5) |
O2W—Na1—O1 | 166.86 (6) | O5—Na1—O3i | 97.80 (5) |
O5—Na1—O1W | 87.51 (5) | O2W—Na1—O3i | 85.57 (5) |
O2W—Na1—O1W | 87.97 (6) | O1—Na1—O3i | 90.33 (5) |
O1—Na1—O1W | 95.25 (6) | O1W—Na1—O3i | 172.76 (6) |
O5—Na1—O3W | 163.62 (6) | O3W—Na1—O3i | 90.36 (5) |
O2W—Na1—O3W | 84.43 (5) |
Symmetry code: (i) −x, −y, −z+2. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···O3Wii | 0.89 | 1.89 | 2.763 (2) | 167.7 |
N1—H1B···O8iii | 0.89 | 1.93 | 2.810 (2) | 170.1 |
N1—H1C···O4iv | 0.89 | 1.91 | 2.7808 (19) | 165.3 |
N2—H2A···O7v | 0.89 | 1.94 | 2.8221 (18) | 168.6 |
N2—H2A···O8v | 0.89 | 2.58 | 3.1815 (18) | 125.6 |
N2—H2B···O3vi | 0.89 | 1.93 | 2.7981 (19) | 165.1 |
N2—H2C···O8vii | 0.89 | 1.86 | 2.750 (2) | 175.2 |
O2—H2···O5 | 0.82 | 1.73 | 2.5491 (17) | 177.0 |
O1W—H1W···O4viii | 0.816 (9) | 2.002 (10) | 2.8150 (19) | 175 (2) |
O2W—H4W···O6iv | 0.818 (9) | 2.024 (11) | 2.8128 (19) | 162 (2) |
O3W—H6W···O1Wix | 0.829 (9) | 1.977 (10) | 2.778 (2) | 162 (2) |
O2W—H3W···O7 | 0.822 (9) | 2.013 (10) | 2.8322 (19) | 174 (2) |
Symmetry codes: (ii) −x+1, −y, −z+2; (iii) x, y−1, z+1; (iv) x+1, y, z; (v) x−1, y, z; (vi) x, y+1, z−1; (vii) −x, −y+2, −z+1; (viii) −x, −y+1, −z+2; (ix) −x+1, −y+1, −z+2. |
Molecular self-assembly of supramolecular architectures has received much attention during recent decades (Kim et al., 2003; Iglesias et al., 2003; Moulton & Zaworotko, 2001). The structures and properties of such systems depend on the coordination and geometric preferences of both the central metals ions and bridging building blocks as well as the influence of weaker non-covalent interactions, such as hydrogen bonds and π-π stacking interactions.
As illustrated in Fig. 1, in the dinuclear centrosymmetric structure of (I) each NaI centre is coordinated by three carboxyl O atoms from three 5-aminoisophthalato ligands, and three water molecules. In the distorted octahedral geometry each of the water molecules is located trans to a carboxyl O atom (Table 1). The Na···Na separation within the centrosymmetric dinuclear complex is 10.251 (3) Å, and the the two central 5-aminoisophthalato ligands are parallel to each other at a plane to plane distance of about 3.43 Å, thus indicating a π stacking interaction (Fig 1). The structure is further extended to a supramolecular network through intra and intermolecular N—H···O and O—H···O hydrogen bonding interactions (Fig 2., Table 2).